CRYSTAL STRUCTURE OF DOUBLE SODIUM-COPPER(II) PARATUNGSTATE B, Na2Cu4[W12O40(OH)2]•22H2O, AND MIXED COPPER (II) PARATUNGSTATE B-HYDROXIDE, Cu5[W12O40(OH)2]•2Cu(OH)2•30H2O

The conditions required for the formation of double sodium-copper(II) paratungstate B Na2Cu4[W12O40(OH)(2)]center dot 22H(2)O (1) and mixed copper(II) paratungstate B-hydroxide Cu-5[W12O40(OH)(2)]center dot 2Cu(OH)(2)center dot 30H(2)O (2) in Cu(NO3)(2) - Na2WO4 - HNO3 - H2O solution acidified up to Z = nu(H+)/nu(WO42-) = 1.29 are determined. The synthesized salts 1 and 2 are examined using chemical analysis, X-ray single crystal analysis, and FTIR spectroscopy. The X-ray single crystal data obtained for compound 1: triclinic, P (1) over bar, a = 11.155(4) angstrom, b = 12.448(4) angstrom, c = 21.979(6) angstrom, alpha = 105.30(3)00B0, beta = 91.99(3)00B0, gamma = 112.51(3)00B0, V = 2687.8(16) angstrom(3) at T = 293 K, Z = 2, d(calc) = 4.419 g/cm(3). The crystal data for 2: triclinic, , a = 10.588(4) angstrom, b = 12.830(4) angstrom, c = 12.852(4) angstrom, alpha = 95.86(3)00B0, beta = 113.65(3)00B0, gamma = 91.76(3)00B0, V = 1586.0(10) angstrom(3) at T = 293 K, Z = 1, d(calc) = 4.119 g/cm(3). In structure 1, Na atoms form distorted octahedra having common vertices with two [W12O40(OH)(2)](10-) anions, and there are three types of coordination polyhedra of Cu atoms: distorted tetragonal bipyramids, trigonal bipyramids, and centrosymmetric rhombic bipyramids. In structure 2, the Cu1, Cu2, and Cu5 atoms are located in the centers of symmetry; their coordination polyhedra are rhombic bipyramids. The anions [W12O40(OH)(2)](10-) are connected by pairs of tetragonal pyramids Cu3O(5) and Cu4O(5) having a common edge of their bases, and their vertices are oriented in opposite directions with respect to the base plane, similarly to the structure of Cu(OH)(2).